CN109518496A - A kind of colouring method of sodolin - Google Patents

A kind of colouring method of sodolin Download PDF

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Publication number
CN109518496A
CN109518496A CN201811451336.4A CN201811451336A CN109518496A CN 109518496 A CN109518496 A CN 109518496A CN 201811451336 A CN201811451336 A CN 201811451336A CN 109518496 A CN109518496 A CN 109518496A
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sodolin
graphene
solution
chitosan
colouring method
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CN109518496B (en
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陈前军
房绍花
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ZHEJIANG JIUCAILONG DYEING AND WEAVING TECHNOLOGY Co.,Ltd.
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Henan Jianfeng Hat Industry Co Ltd
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/20—Physical treatments affecting dyeing, e.g. ultrasonic or electric
    • D06P5/2066—Thermic treatments of textile materials
    • D06P5/2083—Thermic treatments of textile materials heating with IR or microwaves
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
    • D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
    • D06M14/20—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of natural origin
    • D06M14/22—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of natural origin of vegetal origin, e.g. cellulose or derivatives thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/445—Use of auxiliary substances before, during or after dyeing or printing
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/58—Material containing hydroxyl groups
    • D06P3/60—Natural or regenerated cellulose
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30—Flame or heat resistance, fire retardancy properties
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/35—Abrasion, pilling or fibrillation resistance

Abstract

The invention discloses a kind of colouring methods of sodolin, comprising the following steps: Step 1: the compound enzymatic treatment of sodolin；Step 2: sodolin chitose-acrylic amide graft modification；Step 3: graphene layer self assembly；Step 4: microwave dyeing.The colouring method of sodolin provided by the invention, sodolin is handled with complex enzyme liquid, good impurity removing effect, fibre damage is small, by chitosan and acrylamide in sodolin surface graft copolymerization, promote the combination of flax fiber and dye molecule in the progress and dyeing course of surface graphene self assembly, microwave dyeing is easy to operate, mild condition, low energy consumption, it pollutes small, suitable dyes range is wide, dye-uptake is high, it is bright in colour that the present invention dyes gained sodolin, good hand touch, strength and color fastness are high, with good flame retardant property and anti-ultraviolet property, bacteriostasis rate is greater than 99%.

Description

A kind of colouring method of sodolin
Technical field
The present invention relates to technical field of textile printing, and in particular to a kind of colouring method of sodolin.
Background technique
Sodolin has the excellent characteristics such as absorbing sweat, ventilative, dry and comfortable, antiseptic and inhibiting bacteria function, is widely used in textile garment field. The main component of flaxen fiber is cellulose, simultaneously the impurity such as the lignin containing part and hemicellulose, due also to flax fiber Microstructure-crystallinity height, close structure, inclination angle are small etc., cause flax fiber stainability poor, dye-uptake is low, dyefastness Difference, coloured light wither secretly, so the dyeability for improving flaxen fiber is always people's one of the technical problems that are urgent to solve.
Summary of the invention
For the deficiency of existing Dyeing of Linen Fabric method, that the present invention provides a kind of dye-uptakes is high, beautiful in colour, color is firm The Dyeing of Linen Fabric method spent.
The purpose of the present invention is achieved through the following technical solutions:
A kind of colouring method of sodolin, comprising the following steps:
Step 1: the compound enzymatic treatment of sodolin: sodolin is padded in 45 DEG C, the composite enzyme solution of pH value 4~6 After handling 2h, cold water washing takes off and does；
Step 2: sodolin chitose-acrylic amide graft modification: the vinegar for being 1.5% by chitosan and mass fraction Acid solution mixing, electric stirring obtain chitosan solution to being completely dissolved；By chitosan solution and contain the acryloyl of photoinitiator Amine monomers solution is uniformly mixed to obtain polymer fluid, immediately pads the processed sodolin of complex enzyme in polymer fluid, Zhi Houxun Photografting polymerization is carried out in speed merging UV radiation appliance, 100 DEG C of alkali cleanings after the completion of grafting, then it is washed till neutrality with cold water, it dries, obtains Graft modification sodolin；
Step 3: graphene layer self assembly: the graft modification sodolin that step 2 obtains is padded in graphene solution In, 40 DEG C of dipping temperature, dip time 30min, washing dries, dries to obtain graphene self assembly graft modification sodolin；
Step 4: microwave dyeing: the graphene self assembly graft modification sodolin that step 3 obtains being padded dye liquor, is led Enter closed microwave heating chamber, 20min, bath raio 1:30 is dyed with 480W microwave intensity, cold water is washed, soaps after having contaminated.
Further, 12~18U/L of laccase in composite enzyme solution described in step 1,25~30U/L of zytase, pectin 28~32U/L of enzyme, 1.8~2.7g/L of nonionic surfactant.
Further, photoinitiator described in step 2 is 2,4,6- trimethylbenzoy-dipheny phosphine oxides (TPO)。
It further, also include crosslinking agent, pore-foaming agent in polymer fluid described in step 2；The crosslinking agent is metering system One of amide, N,N methylene bis acrylamide, divinylbenzene, Ethylene-glycol-dimethacrylate are a variety of；The pore Agent is one of polyvinylpyrrolidone, polyethylene glycol, water soluble surfactant active, inert fluid or a variety of.
Further, the mass fraction of chitosan is 1~2% in polymer fluid described in step 2, acrylamide monomer Mass fraction is 6~10%, and the mass fraction of initiator is 0.5~1%.
Further, chitosan described in step 2 is nanometer degradation chitosan, and particle size range is 100~500nm；
Further, lye used in alkali cleaning is 0.1mol/L sodium hydroxide solution in step 2.
Further, graphene solution described in step 3 is the aqueous solution that graphene is configured to 1mg/L first, then PH is adjusted to alkalinity with sodium hydroxide solution, and graphene carboxylated is obtained into the electronegative graphene solution in surface with monoxone.
Further, dye dosage 2% (owf), rare-earth Gd Cl in dye liquor described in step 43Dosage 0.1% (owf), Middle dyestuff can be used any in reactive dye, direct dyes and the dye of positive ion.
Contain hydrolase pectase and zytase in composite enzyme solution used in the present invention, there are also oxidoreducing enzyme laccase, For the characteristic of sodolin, these three enzymes are subjected to rational proportion, it, can be effective under 45 DEG C, the optimal conditions of pH value 4~6 Hemicellulose, pectin and lignin are removed, the wetability of sodolin can be significantly improved, fabric strength damage is small.
The present invention passes through light-initiated chitosan and acrylamide in sodolin surface graft copolymerization, in atmospheric air i.e. It can occur, it is easy to operate, it is at low cost；When sodolin is padded into polymer fluid, the small chitosan of molecular weight is quickly entered in fiber Portion, the amino of protonation can be reduced the negative electrical charge of fiber institute band in conjunction with sodolin, promote dyestuff to the affine of fiber Power, photoinitiator splits into free radical after absorbing the radiation energy of ultraviolet light, then by radical transfer to cellulose macromolecule, from And cause acrylamide and graft polymerization reaction occurs on sodolin surface, the big chitosan of molecular weight and acrylamide occur altogether It is poly-, it is interspersed in sodolin surface, a part of dye molecule can be combined first with acrylamide and chitosan macromolecular, and a part is thoroughly The hole for crossing copolymer enters fibrous inside in conjunction with the chitosan small molecule of fiber surface, improves the dye-uptake of sodolin.
One layer of graphene of sodolin outer layer self assembly of the present invention, amido and graphene on chitosan and polyacrylamide Van der Waals force, hydrogen bond between the carboxyl on surface, ionic bond are the driving forces of self assembly, can be improved graphene in flax fiber table The adsorbance and binding strength in face, when dyeing, graphene can adsorb rapidly the dye molecule in dye liquor, improve dyeing efficiency, In addition, graphene plays an important role to the raising of sodolin color fastness and intensity raising.
The present invention uses microwave dyeing, and the energy of microwave is absorbed by hydrone and dye molecule, in the high frequency of quick alternation Under electromagnetic field effect, the orientation of these polar molecules quickly changes with the variation of electromagnetic field, promotes friction life between polar molecule Heat, temperature condition is more uniform, chemical group can selective absorbing microwave, it is poly- to can be improved dye molecule and graphene, shell The affinity of sugar, acrylamide, flax fiber improves dye-uptake and degree of fixation, improves the intensity of flax fiber.
Compared with the prior art, the invention has the following beneficial effects:
(1) present invention handles sodolin with complex enzyme liquid, and the increasing of nonionic surfactant and complex enzyme is utilized Effect effect, treatment conditions are mild, and the time is short, small to flax fiber damage, most of impurity can be effectively removed, without using burning Alkali, avoid coloured light in Dyeing of Linen Fabric caused by impurity, chemical damage wither dark, poor color fastness, color is shallow and dyeing defect, The problems such as color difference；
(2) present invention is obtained by chitosan and acrylamide in sodolin surface graft copolymerization on sodolin surface The perforated membrane interted to one layer of chitosan, the porous structure of the good biocompatibility of chitosan, water imbibition and copolymer make Flax fiber has good gas permeability, overcome it is simple it is acrylic amide modified caused by the defect that is deteriorated of feel, pass through simultaneously The sodolin initial decomposition temperature crossed after copolymerized grafting decreases, be grafted the carbon yield of later sodolin by 9.14% has been increased to 18.24%, illustrates to slow down the heating rate of sodolin after grafting, and facilitate the shape of layer of charcoal At being improved the flame retardant property of fabric, N element, the N that when burning generates be rich in acrylamide2Inert gas makes fabric Burning zone ambient oxygen concentration reduces, and inhibits the lasting progress of burning；
(3) present invention carries out graphene self assembly again on chitosan and acrylic amide graft copolymerization layer, and driving force is much Greater than the self assembly directly on sodolin, the adsorbance and binding strength of graphene are greatly promoted, and graphene is uniformly distributed And by hydrogen bond be equal to flax fiber, chitosan, acrylamide interaction, significantly improve sodolin thermal stability and Mechanical property makes sodolin have the good anti-purple outer performance of line, while compared with the direct coating sodolin of graphene, this The sodolin that invention dyeing obtains has better wear-resisting, wears performance, in addition, can be in fabric surface shape after graphene burning At one layer of fine and close layer of charcoal, obstruct contact of the air with fiber, further promote flame retardant property, at the same graphene also with chitosan Collaboration plays antibiotic effect；
(4) in dyeing course of the present invention, the high specific surface of porous structure, the graphene of sodolin surface graft copolymerization object Product is that effective adsorpting dye molecule, dye molecule enter fibrous inside, provide conveniently, and the metal ion of added rare earth chloride can be with Fiber, modification by copolymerization layer, the carboxyl on graphene, amino groups and hydroxyl, amino on dye molecule etc. are complexed, In addition microwave dyeing energy transmission is fast, can reduce the dyeing process time, so as to effectively promote dye utilization rate and color fastness, with Existing high-temperature pressure dyeing method is compared, easy to operate, reduces dyestuff and auxiliary dosage, and waste water generates less, can reduce and be coloured to This, mitigates environmental pollution.
Specific embodiment
Further to illustrate technological means and its effect adopted by the present invention, below according to preferred implementation of the invention Example is described in detail.
Embodiment 1
A kind of colouring method of sodolin, comprising the following steps:
Step 1: the compound enzymatic treatment of sodolin: sodolin is padded in 45 DEG C, the composite enzyme solution of pH value 4~6 After handling 2h, cold water washing takes off and does；
Step 2: sodolin chitose-acrylic amide graft modification: the vinegar for being 1.5% by chitosan and mass fraction Acid solution mixing, electric stirring obtain chitosan solution to being completely dissolved；By chitosan solution and contain photoinitiator 2,4,6- tri- Methyl benzoyl-diphenyl phosphine oxide (TPO), acrylamide monomer, crosslinking agent Methacrylamide, pore-foaming agent polyethylene pyrrole The solution of pyrrolidone is uniformly mixed to obtain polymer fluid, immediately pads the processed sodolin of complex enzyme in polymer fluid, later Photografting polymerization is carried out in merging UV radiation appliance rapidly, UV energy is 0.60J/cm2, grafting after the completion of with 100 DEG C, The washing of 0.1mol/L sodium hydroxide solution, then it is washed till neutrality with cold water, it dries, obtains graft modification sodolin；
Step 3: graphene layer self assembly: the graft modification sodolin that step 2 obtains is padded in graphene solution In, 40 DEG C of dipping temperature, dip time 30min, washing dries, dries to obtain graphene self assembly graft modification sodolin；
Step 4: microwave dyeing: the graphene self assembly graft modification sodolin that step 3 obtains being padded dye liquor, is led Enter closed microwave heating chamber, 20min, bath raio 1:30 is dyed with 480W microwave intensity, cold water is washed, soaps after having contaminated.
Further, laccase 12U/L in composite enzyme solution described in step 1, zytase 25U/L, pectase 28U/L, Paregal O 1.8g/L.
Further, the mass fraction of chitosan is 1% in polymer fluid described in step 2, the quality of acrylamide monomer Score is 6%, and the mass fraction of initiator is 0.5%.
Further, chitosan described in step 2 is nanometer degradation chitosan, and particle size range is 100~500nm；
Further, graphene solution described in step 3 is the aqueous solution that graphene is configured to 1mg/L first, then PH is adjusted to alkalinity with sodium hydroxide solution, and graphene carboxylated is obtained into the electronegative graphene solution in surface with monoxone.
Further, dye dosage 2% (owf), rare-earth Gd Cl in dye liquor described in step 43Dosage 0.1% (owf), Middle dyestuff uses reactive dye.
Embodiment 2
A kind of colouring method of sodolin, comprising the following steps:
Step 1: the compound enzymatic treatment of sodolin: sodolin is padded in 45 DEG C, the composite enzyme solution of pH value 4~6 After handling 2h, cold water washing takes off and does；
Step 2: sodolin chitose-acrylic amide graft modification: the vinegar for being 1.5% by chitosan and mass fraction Acid solution mixing, electric stirring obtain chitosan solution to being completely dissolved；By chitosan solution and contain photoinitiator 2,4,6- tri- Methyl benzoyl-diphenyl phosphine oxide (TPO), acrylamide monomer, crosslinking agent N,N methylene bis acrylamide, pore-foaming agent The solution of polyethylene glycol is uniformly mixed to obtain polymer fluid, immediately pads the processed sodolin of complex enzyme in polymer fluid, it Carry out photografting polymerization in merging UV radiation appliance rapidly afterwards, UV energy is 0.65J/cm2, grafting after the completion of with 100 DEG C, The washing of 0.1mol/L sodium hydroxide solution, then it is washed till neutrality with cold water, it dries, obtains graft modification sodolin；
Step 3: graphene layer self assembly: the graft modification sodolin that step 2 obtains is padded in graphene solution In, 40 DEG C of dipping temperature, dip time 30min, washing dries, dries to obtain graphene self assembly graft modification sodolin；
Step 4: microwave dyeing: the graphene self assembly graft modification sodolin that step 3 obtains being padded dye liquor, is led Enter closed microwave heating chamber, 20min, bath raio 1:30 is dyed with 480W microwave intensity, cold water is washed, soaps after having contaminated.
Further, laccase 15U/L in composite enzyme solution described in step 1, zytase 28U/L, pectase 30U/L, JFC 2.3g/L。
Further, the mass fraction of chitosan is 1.5% in polymer fluid described in step 2, the matter of acrylamide monomer Measuring score is 8%, and the mass fraction of initiator is 0.8%.
Further, chitosan described in step 2 is nanometer degradation chitosan, and particle size range is 100~500nm；
Further, graphene solution described in step 3 is the aqueous solution that graphene is configured to 1mg/L first, then PH is adjusted to alkalinity with sodium hydroxide solution, and graphene carboxylated is obtained into the electronegative graphene solution in surface with monoxone.
Further, dye dosage 2% (owf), rare-earth Gd Cl in dye liquor described in step 43Dosage 0.1% (owf), Middle dyestuff uses direct dyes.
Embodiment 3
A kind of colouring method of sodolin, comprising the following steps:
Step 1: the compound enzymatic treatment of sodolin: sodolin is padded in 45 DEG C, the composite enzyme solution of pH value 4~6 After handling 2h, cold water washing takes off and does；
Step 2: sodolin chitose-acrylic amide graft modification: the vinegar for being 1.5% by chitosan and mass fraction Acid solution mixing, electric stirring obtain chitosan solution to being completely dissolved；By chitosan solution and contain photoinitiator 2,4,6- tri- Methyl benzoyl-diphenyl phosphine oxide (TPO), acrylamide monomer, crosslinking agent divinylbenzene, dimethacrylate second two Ester, pore-foaming agent water soluble surfactant active, inert fluid solution be uniformly mixed to obtain polymer fluid, it is immediately that complex enzyme is processed Sodolin pads in polymer fluid, carries out photografting polymerization in merging UV radiation appliance rapidly later, and UV energy is 0.70J/ cm2, washed after the completion of grafting with 100 DEG C, 0.1mol/L sodium hydroxide solution, then be washed till neutrality with cold water, dry, obtain grafting and change Property sodolin；
Step 3: graphene layer self assembly: the graft modification sodolin that step 2 obtains is padded in graphene solution In, 40 DEG C of dipping temperature, dip time 30min, washing dries, dries to obtain graphene self assembly graft modification sodolin；
Step 4: microwave dyeing: the graphene self assembly graft modification sodolin that step 3 obtains being padded dye liquor, is led Enter closed microwave heating chamber, 20min, bath raio 1:30 is dyed with 480W microwave intensity, cold water is washed, soaps after having contaminated.
Further, laccase 18U/L in composite enzyme solution described in step 1, zytase 30U/L, pectase 32U/L, Foretell public Tea Saponin 2.7g/L.
Further, the mass fraction of chitosan is 2% in polymer fluid described in step 2, the quality of acrylamide monomer Score is 10%, and the mass fraction of initiator is 1%.
Further, chitosan described in step 2 is nanometer degradation chitosan, and particle size range is 100~500nm；
Further, graphene solution described in step 3 is the aqueous solution that graphene is configured to 1mg/L first, then PH is adjusted to alkalinity with sodium hydroxide solution, and graphene carboxylated is obtained into the electronegative graphene solution in surface with monoxone.
Further, dye dosage 2% (owf), rare-earth Gd Cl in dye liquor described in step 43Dosage 0.1% (owf), Middle dyestuff uses the dye of positive ion.
Comparative example 1
Except polymer fluid is not in addition to chitosan-containing in step 2, remaining is the same as embodiment 3.
Comparative example 2
Except step 3 is not carried out, i.e., the graft modification sodolin that step 2 obtains does not carry out outside graphene self assembly, Remaining same embodiment 3.
Comparative example 3
Except rare-earth Gd Cl is not added in step 43Outside, remaining is the same as embodiment 3.
Comparative example 4
In addition to step 4 is using conventional dyeing process, remaining is the same as embodiment 3.
Performance test
Following performance test carried out to Examples 1 to 3 and the resulting sodolin of comparative example 1~4 respectively, test method and As a result as follows:
1 fabric strength
Fabric strength is by GB/T 3923-1997 " textile fabric tensile property " on YG026M-250 strength tester Measurement, as a result such as table 1.
1 Examples 1 to 3 of table, 1~4 gained sodolin strength of comparative example
As it can be seen from table 1 the strength of sodolin obtained by Examples 1 to 3 to broadwise far beyond existing flax through knitting The strength of object is horizontal, and comparative example 1,2,4 sodolin strength has different degrees of decline compared with embodiment, this is because right The not chitosan-containing of ratio 1, the load capacity of graphene and binding strength are not as good as embodiment, the not containing graphene Iy self-assembled layer of comparative example 2, Sodolin strength declines to a great extent, and comparative example 4 uses conventional dyeing process, since the temperature of conventional dyeing process is high, examination used Agent is strong to the destructiveness of flax fiber, and sodolin strength is caused to decline, and rare-earth Gd Cl is not added in comparative example 33, sodolin is strong Power changes less compared with embodiment.
The measurement of 2 dye-uptakes
The absorbance A of former dye liquor is surveyed in maximum absorption wave strong point0, measure the absorbance A for changing over time dye extraction raffinaten, and press Following formula seeks the dye-uptake for calculating fabric.
Dye-uptake E (%)=(1-An/A0) × 100%
A in formulan: contaminate the absorbance of extraction raffinate；A0: contaminate the absorbance of stoste.Measurement result such as table 2.
2 Examples 1 to 3 of table, 1~4 gained sodolin dye-uptake of comparative example
Project Dye-uptake (%)
Embodiment 1 94.1
Embodiment 2 93.9
Embodiment 3 95.6
Comparative example 1 72.4
Comparative example 2 78.8
Comparative example 3 82.5
Comparative example 4 50.2
From table 2 it can be seen that sodolin dye-uptake obtained by Examples 1 to 3 is all larger than 90%, 1~4 flax of comparative example is knitted Object dye-uptake has different degrees of decline compared with embodiment, this is because chitosan-containing, flax fiber do not adsorb comparative example 1 The amount of dye molecule is not as good as embodiment, the not containing graphene Iy self-assembled layer of comparative example 2, the rate of adsorption of the sodolin to dye molecule Decline, identical dyeing time, adsorbed dye molecule are considerably less than embodiment, and rare-earth Gd Cl is not added in comparative example 33, dyestuff The binding capacity of molecule is reduced, and comparative example 4 uses conventional dyeing process, since impurity exists in flax fiber and microstructure is special Point causes sodolin dye-uptake low.
The test of 3 color fastness
It is resistance to soap with colour fastness to rubbing respectively according to " the resistance to color jail of soaping of textile color stability test GB/T3921-2008 Degree " and GB/T3920-2008 " textile color stability test colour fastness to rubbing " tested, as a result such as table 3.
3 Examples 1 to 3 of table, 1~4 gained sodolin color fastness test result of comparative example
From table 3 it can be seen that sodolin color fastness obtained by Examples 1 to 3 is higher, 1~4 sodolin color jail of comparative example Degree has compared with embodiment and largely declines, this is because the not chitosan-containing of comparative example 1, flax fiber dye molecule Binding strength is not as good as embodiment, and the adsorption capacity of dye molecule does not drop to comparative example 2 in containing graphene Iy self-assembled layer, sodolin Low, rare-earth Gd Cl is not added in comparative example 33, there is no the complexings with dye molecule, are deteriorated with the binding force of dye molecule, right Ratio 4 uses conventional dyeing process, due to impurity presence and microstructure feature in flax fiber, causes sodolin color fastness It is low.
4 uvioresistant performances
Using textile fabric ultraviolet protection performance tester test gained fabric UPF value, every piece sample testing 8 times, take Average value the results are shown in Table 4.
4 Examples 1 to 3 of table, 1~4 gained sodolin uvioresistant performance test result of comparative example
Project UPF UVA UVB
Embodiment 1 75 34 16
Embodiment 2 72 38 16
Embodiment 3 78 35 14
Comparative example 1 62 70 37
Comparative example 2 26 86 42
Comparative example 3 55 42 23
Comparative example 4 23 89 30
From table 4, it can be seen that sodolin uvioresistant performance obtained by Examples 1 to 3 is preferable, 1,2,4 flax of comparative example is knitted Object uvioresistant performance has different degrees of decline compared with embodiment, this is because the not chitosan-containing of comparative example 1, graphene from For the binding strength of assembled layers not as good as embodiment, the not containing graphene Iy self-assembled layer of comparative example 2 reduces the absorbability of ultraviolet light, Comparative example 4 uses conventional dyeing process, and dyeing course may cause graphene and fall off, and causes uvioresistant performance to decline, comparative example 3 Rare-earth Gd Cl is not added3, ultraviolet absorption ability is influenced little.
5 bacteriostasis rates
Antibacterial calibration is carried out using GB/T20944.3-2008 " the evaluation third portion of antibacterial textile performance: succusion " Examination is measured, using color fastness to washing testing machine washing methods, the bacteriostasis rate of the sodolin after testing washing 5 times, test result Such as table 5.
5 Examples 1 to 3 of table, 1~4 gained sodolin uvioresistant performance test result of comparative example
Project Bacteriostasis rate (%) Bacteriostasis rate (%) after washing 10 times
Embodiment 1 99.5 78.6
Embodiment 2 99.7 77.2
Embodiment 3 99.8 69.3
Comparative example 1 76.7 51.5
Comparative example 2 63.5 34.6
Comparative example 3 99.2 64.7
Comparative example 4 73.9 49.1
As can be seen from Table 5, sodolin bacteriostasis rate and washability obtained by Examples 1 to 3 are preferable, and comparative example 1,2,4 is sub- Linen uvioresistant performance has different degrees of decline compared with embodiment, this is because the not chitosan-containing of comparative example 1, causes Biocidal property is decreased obviously, along with the binding strength of graphene Iy self-assembled layer is not as good as embodiment, therefore bacteriostasis rate fall compared with Greatly, the not containing graphene Iy self-assembled layer of comparative example 2, causes biocidal property and washability to be decreased obviously, and comparative example 4 uses normal dyeing work Skill, dyeing course may cause graphene and fall off, and biocidal property is caused to be decreased obviously, and rare-earth Gd Cl is not added in comparative example 33, to antibacterial Capacity is little, suitable with embodiment bacteriostasis rate, but due to the missing of complexing, washability is caused to be deteriorated, washing 10 Bacteriostasis rate has dropped 34.8% after secondary.
To sum up, the colouring method of sodolin provided by the invention, easy to operate, mild condition, low energy consumption, pollution is small, Suitable dyes range is wide, and dye-uptake is high, and gained sodolin is bright in colour, good hand touch, strongly with color fastness height, has good Flame retardant property and anti-ultraviolet property, bacteriostasis rate are greater than 99%.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, ability Other modifications or equivalent replacement that domain those of ordinary skill makes technical solution of the present invention, without departing from skill of the present invention The spirit and scope of art scheme, are intended to be within the scope of the claims of the invention.

Claims (9)

1. a kind of colouring method of sodolin, which comprises the following steps:
Step 1: the compound enzymatic treatment of sodolin: sodolin being padded and is handled in 45 DEG C, the composite enzyme solution of pH value 4 ~ 6 After 2 h, cold water washing takes off and does；
Step 2: sodolin chitose-acrylic amide graft modification: the acetum for being 1.5% by chitosan and mass fraction Mixing, electric stirring obtain chitosan solution to being completely dissolved；By chitosan solution and contain the acrylamide monomer of photoinitiator Solution is uniformly mixed to obtain polymer fluid, immediately pads the processed sodolin of complex enzyme in polymer fluid, later merging rapidly Photografting polymerization is carried out in UV radiation appliance, 100 DEG C of alkali cleanings after the completion of grafting, then it is washed till neutrality with cold water, it dries, must be grafted Modified sodolin；
Step 3: graphene layer self assembly: the graft modification sodolin that step 2 obtains being padded in graphene solution, is soaked 40 DEG C of stain temperature, 30 min of dip time, washing dries, dries to obtain graphene self assembly graft modification sodolin；
Step 4: microwave dyeing: the graphene self assembly graft modification sodolin that step 3 obtains being padded dye liquor, is imported close The microwave heating chamber closed dyes 20 min, bath raio 1:30 with 480 W microwave intensities, and cold water is washed, soaps after having contaminated.
2. a kind of colouring method of sodolin according to claim 1, which is characterized in that complex enzyme described in step 1 12 ~ 18 U/L of laccase in solution, 25 ~ 30 U/L of zytase, 28 ~ 32 U/L of pectase, nonionic surfactant 1.8 ~ 2.7 g/L。
3. a kind of colouring method of sodolin according to claim 1, which is characterized in that light-initiated described in step 2 Agent is 2,4,6- trimethylbenzoy-dipheny phosphine oxide (TPO).
4. a kind of colouring method of sodolin according to claim 1, which is characterized in that polymer fluid described in step 2 In also include crosslinking agent, pore-foaming agent；The crosslinking agent be Methacrylamide, N,N methylene bis acrylamide, divinylbenzene, One of Ethylene-glycol-dimethacrylate is a variety of；The pore-foaming agent is polyvinylpyrrolidone, polyethylene glycol, water-soluble table One of face activating agent, inert fluid are a variety of.
5. a kind of colouring method of sodolin according to claim 1, which is characterized in that polymer fluid described in step 2 The mass fraction of middle chitosan is 1 ~ 2%, and the mass fraction of acrylamide monomer is 6 ~ 10%, the mass fraction of initiator is 0.5 ~ 1%。
6. a kind of colouring method of sodolin according to claim 1, which is characterized in that chitosan described in step 2 is Nanometer degradation chitosan, particle size range are 100 ~ 500 nm.
7. a kind of colouring method of sodolin according to claim 1, which is characterized in that alkali used in alkali cleaning in step 2 Liquid is 0.1 mol/L sodium hydroxide solution.
8. a kind of colouring method of sodolin according to claim 1, which is characterized in that graphene described in step 3 Solution is the aqueous solution that graphene is configured to 1 mg/L first, then adjusts pH to alkalinity with sodium hydroxide solution, uses chloroethene Graphene carboxylated is obtained the electronegative graphene solution in surface by acid.
9. a kind of colouring method of sodolin according to claim 1, which is characterized in that contaminated in dye liquor described in step 4 Expect dosage 2% (owf), rare-earth Gd Cl3Dosage 0.1% (owf), wherein reactive dye, direct dyes and cation can be used in dyestuff It is any in dyestuff.
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